CN105331387A - Technological method for preparing aviation fuel through biomass thermal catalytic conversion and refining - Google Patents
Technological method for preparing aviation fuel through biomass thermal catalytic conversion and refining Download PDFInfo
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Abstract
The invention discloses a technological method for preparing aviation fuel through biomass thermal catalytic conversion and refining. The method comprises the following steps that 1, biomass is converted into stable biomass oil with a single oxygen-containing functional group as the feature through a thermal catalytic conversion method; 2, a carbon-carbon key formation reaction is designed, the carbon chain length of the stable biomass oil is adjusted, and an aviation fuel precursor with the carbon chain length meeting the biological aviation fuel requirements is obtained; 3, hydrodeoxygenation is performed on the aviation fuel precursor to prepare the biological aviation fuel conforming to aviation fuel indexes. By the adoption of the technological way, starting from lignocellulose such as straw, and the aviation fuel yield can reach 20%. The obtained aviation fuel product can completely conform to jet-A level aviation fuel standards. The method has the advantages that the raw material source is wide, the features of biomass raw materials are sufficiently considered, and the aviation fuel is high in yield and grade.
Description
Technical field
The invention belongs to renewable aviation fuel and biomass utilization technologies field, particularly relate to the aviation fuel products that the preparation such as the renewable biomass resource that utilizes agricultural crop straw, trees branch, energy crop (plant) meets existing aviation fuel standard.
Background technology
Along with developing rapidly of Civil Aviation Industry, the demand of aviation fuel also constantly increases.For China, within 2011, China Aviation kerosene consumption is more than 1,800 ten thousand tons, occupies second place of the world, and by with annual more than 10% speed increment.Based on reality and the oil refining industrial structure of a large amount of import of Chinese crude oil, for ensureing the stable supplying of aviation fuel, the aviation fuel source outside necessary search for oil.
On the other hand, air system is also faced with huge environmental protection pressure, carbon dioxide discharge-reduction become each airline must faced by a difficult problem.As the region that aviation carbon tax is implemented at first, European Union determined from 2012, the commercial airliner greenhouse gas emission total amount dropped in European Union region is limited in 97% of 2004 ~ 2006 yearly mean levels, within 2013, be down to 95%, and huge carbon emission expense is imposed to each airline exceeding limit.According to statistics, only 2012 Nian Ge airlines cause cost to increase by 2,400,000,000 Euros because of carbon emission expense.In the long run, maintenance is continued ascendant trend and may be generalized to other regions in the world by aviation carbon tax.
The aviation fuel that bio-aviation fuel is is raw material production with renewable biomass resource, does not produce carbon emission in its Life cycle.Contribute to the dual difficult problem solving Aerobiz fuel crunch and carbon dioxide discharge-reduction.Therefore the exploitation of countries in the world to bio-aviation fuel is paid much attention to, and promotes the researchs such as bio-aviation fuel production, standard foundation and seaworthiness detection and carries out in a large number.
Up to now, the exploitation of bio-aviation fuel is still at the initial stage, still there is associated bottleneck in the application of its heavy industrialization: 1) existing bio-aviation fuel technology of preparing relies on higher-grade biomass resource (high-quality grease) and the expensive course of processing (hydrogenation deoxidation), causes its production cost too high; 2) the extensive of raw material continues the scale operation that deliverability also limits bio-aviation fuel.Therefore, the lignocellulose-like biomass (as stalk etc.) that can extensively obtain is converted into aviation fuel expeditiously, is very attractive technological line.
Be oxygen-free, C by hydrophilic, solid-state Biomass
9-C
14aviation kerosene molecule need to experience the profound change in phase and chemical constitution, also need the Areal Distribution considering biomass simultaneously.Biomass pyrolytic utilizes chemical bond in heat collapse biomass, carry out component recombination, from solid-state biomass, high-level efficiency obtains the process of liquid bio oil, and can realize distributed production, be the leading technology of biomass economy great potential, be the primary study direction in biomass energy field always.
The early stage research of biomass pyrolytic is to produce product liquid to greatest extent for major objective, take reactor development as characteristic, define fluidized-bed reactor (Dynamotive, Canada), circulating fluid bed reactor (Ensyn), rotating cone reactor (BTG, Universiteit Twente, Holland) and the biomass pyrolysis device that differs from one another such as cyclonic reactor (NREL, the U.S.).Wherein Dutch BTG and Canadian Dynamotive company have built up the pyrolysis industrial demonstration unit processing 50 tons and 100 tons biomass day respectively, and bio oil productive rate is all more than 60%.China starts biomass pyrolytic research the nineties in last century, Agricultural University Of Shenyang's nineteen ninety-five introduces a set of rotating cone fast pyrogenation testing apparatus from Holland, carry out biomass pyrolysis liquefaction technical study, thereafter the school such as China Science & Technology University, Zhejiang University and R&D institution have also carried out extensive work in this direction, and portion of techniques has entered pilot scale demonstration phase.
Because quality of bio-oil (composition complexity, High water cut, unstable chemcial property etc.) is lower, marketing receives very big restriction, also limit biomass pyrolytic technology and really moves towards industry application from Industrial demonstration scale.Therefore from the beginning of this century, the research focus in biomass pyrolytic direction starts to turn to the bio oil grade lifting process to obtain for the purpose of higher-grade fuel and chemical.Along with research is goed deep into, scientists finds that bio oil is often subject to the puzzlement that bio oil repolymerization produces a large amount of semicoke class material in grading process.The research of European Union the 6th framework " in petroleum refining process co-processing improving quality of bio oil " project and the U.S. " national advanced biofuel alliance " project all shows, carry out mild hydrogenation to bio oil, the coke forming property of suppression bio oil is the key of bio oil success upgrading.Inspire by this, the research of biomass pyrolytic enters the new stage obtaining stabilate oil, the new pyrolysis form such as catalytic pyrolysis of biomass is paid close attention to, contacting of the fields such as biomass through pyrolysis process and refining of petroleum is also increasingly tight, and the famous oil company such as UOP, Shell plays a significant role in this field gradually.
By the low-grade restriction of bio oil, the rare report being prepared aviation fuel by biomass pyrolytic route at present.In existing bio oil upgrading work, in gained fuel, the selectivity of aviation fuel is very low.The result of study in U.S.'s northwest Pacific laboratory shows, in bio oil hydrogenation products, the highest yield of aviation fuel is only 40%, gained aviation fuel based on aromatic compounds, and carries out hydrogenation to the bio oil containing a large amount of oxygen and also causes the hydrogen consumption of this technological process up to >800NL/kg raw material.
In sum, prepare aviation fuel from biomass by pyrolysis route and still there is following difficulty and challenge: the green coke characteristic in the low-grade and grading process of 1) bio oil; 2) low aviation fuel selectivity and be confined to aromatic hydrocarbon aviation fuel composition; 3) high hydrogen consumption and the cost caused thus and safety problem.
Summary of the invention
In view of this, the invention reside in and provide a kind of aviation fuel mass yield high and gained aviation fuel meets the biomass thermal catalyzed conversion of jet-A aviation fuel standard and prepares the processing method of aviation fuel.
The present invention is achieved through the following technical solutions: biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, comprises the steps:
(1) thermocatalysis method for transformation is utilized to be with single oxygen-containing functional group stabilate oil that is feature by Wood Adhesives from Biomass;
(2) design C-C formation reaction, regulate the carbon chain lengths of described stabilate oil, obtain the aviation fuel presoma that carbon chain lengths meets bio-aviation fuel requirement;
(3) described aviation fuel presoma hydrogenation deoxidation preparation meets the bio-aviation fuel of aviation fuel index.
Above-mentioned biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, in step (1): the catalyzer used in thermocatalysis method for transformation is zeolite molecular sieve, one or more in variable valent metal oxide compound and transition metal salt; Temperature of reaction is 300 DEG C-600 DEG C, and reactor types is the pyrolysis form [reactor is fluidized-bed or rotating cone] of accessible site catalyzer.
Above-mentioned biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, in step (1): temperature of reaction is 400 DEG C-500 DEG C.
Above-mentioned biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, in step (2): the hydrogenation-alkylated reaction utilizing oxygen-containing functional group to participate in and/or aldol reaction, the carbochain realizing described stabilate oil increases.
Above-mentioned biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, in step (2): the catalyzer of carbochain reaction of propagation is solid acid catalyst or liquid acid catalyst, and temperature of reaction is 20 DEG C-200 DEG C.
Above-mentioned biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, in step (2): described solid acid catalyst is zeolite molecular sieve or ion exchange resin, described liquid acid catalyst is sulfuric acid, and temperature of reaction is 60 DEG C-200 DEG C.
Above-mentioned biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, in step (3): described aviation fuel presoma hydrogenation deoxidation process is petrochemical complex diesel oil hydrogenation workshop section, and catalyzer is Ni-Mo/Al
2o
3, Co-Mo/Al
2o
3with one or more in supported precious metal catalyst.
Above-mentioned biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, in step (3): in hydrogenation deoxidation process, catalyzer is respectively Pt/C and Co-Mo/Al
2o
3mixture, Pt/C and Co-Mo/Al
2o
3mass ratio be the mass ratio of 1:1, Pt and C be 0.01:1, Co/Mo and Al
2o
3mass ratio be 0.02/0.03:1; Reactor inlet temperature is 120 DEG C, and temperature out is 320 DEG C, and reaction pressure is 5Mpa.
Above-mentioned biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, by aviation fuel presoma hydrogenation deoxidation described in the carbon chain lengths of stabilate oil described in single stage method completing steps (2) and step (3).
Above-mentioned biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, in the reaction by aviation fuel presoma hydrogenation deoxidation described in the carbon chain lengths of stabilate oil described in single stage method completing steps (2) and step (3), the catalyzer of use is any one in the mesoporous KA of mesoporous Betazeolite and Pt/ of Pd/ or the mixture of the two.
The invention has the beneficial effects as follows: for the active demand of bio-aviation fuel and the technological challenge of biomass pyrolytic aviation fuel route, the present invention, on the basis retaining the advantages such as the distributed production of biomass pyrolytic, proposes the bio-aviation fuel syntheti c route based on biomass thermal catalyzed conversion and upgrading.Concrete steps comprise: (1) balance biomass pyrolytic oil-proofness, carbon yield and follow-up carbon number adjustment demand, are the stabilate oil that is feature with single oxygen-containing functional group by thermocatalysis method for transformation by Wood Adhesives from Biomass; (2) utilize oxygen-containing functional group in bio oil, design C-C formation reaction (as shown in Figure 1 and Figure 4), stabilate oil is converted into the aviation fuel presoma that carbon chain lengths meets bio-aviation fuel requirement; (3) hydrogenation deoxidation means are adopted aviation fuel presoma to be changed into the bio-aviation fuel meeting aviation fuel index.
The present invention adjusts target organism oil molecule and the thermocatalysis transformation routes of demand by design balance biomass pyrolytic oil-proofness, carbon yield and follow-up carbon number, realize preparing from biomass the stabilate oil that single oxygen-containing functional group is feature, described stabilate oil comprises the oxygen containing oxygenatedchemicals of all kinds of list (single phenols, furans, ketone, aldehydes) etc.
Use present invention process route, from biomass such as lignocellulose such as stalks, aviation fuel mass yield can reach 20%.Gained aviation fuel products can meet the aviation fuel standards such as jet-A completely.The method have raw material sources extensively, take into full account that biomass material feature, aviation fuel yield are high, grade advantages of higher.
Accompanying drawing explanation
Fig. 1: stabilate oil carbon chain adjustment reaction schematic diagram (phenols);
Fig. 2: ZSM-5 molecular sieve catalyzer scanning electron microscope (SEM) photograph;
A place enlarged view in Fig. 3: Fig. 2;
Fig. 4: stabilate oil carbon chain adjustment reaction schematic diagram (furans).
Embodiment
Embodiment 1:
The present embodiment use biomass material be pre-dry pine wood chip (moisture content <10wt%), use catalyzer for ZSM-5 zeolite molecular sieve (its scanning electron microscope (SEM) photograph as shown in Figures 2 and 3).Thermocatalysis conversion process is carried out in a fluidized bed reactor.In reaction process, 200g catalyzer is joined in fluidized-bed, and adopt nitrogen fluidisation to form bubbling bed reactor.Then biomass are incorporated in fluidized-bed by feeding screw, and the speed that biomass are incorporated into fluidized-bed is 100g/h, in 550 DEG C, thermocatalysis conversion reaction occur.The pyrolysis oil gas generated in fluidized-bed enters in condenser and carries out condensation recovery after cyclonic separator separate ash and the catalyzer that carries, uses the condensation of one-level deep cooling to reclaim and to obtain stabilate oil.Gained stabilate oil, except keeping sample analysis, provides follow-up upgrading to react and uses.Pyrolysis product distribution and gained stabilate oil properties and chemical constitution are as shown in table 1 and table 2.Can find from table 1 compared with comparative example 1, in gained stabilate oil, oxygen level obviously reduces.Can to find from table 2 in gained stabilate oil that oxygenatedchemicals is mainly phenols and non-phenols fragrance containing materials such as oxygen classes further, the bio oil molecule of many oxygen-containing functional groups features such as carbohydrate is by complete reaction.
In the present embodiment, the carbochain adjustment of stabilate oil and hydrogenation deoxidation adopt that single stage method is integrated carries out.Upgrading reaction is carried out in the high pressure fixed-bed reactor of continuous flow, and stabilate oil pumps into high pressure fixed-bed reactor by accurate fresh feed pump, reacts with the catalyzer generation catalysis upgrading being positioned at constant temperature zone.The mixture of mesoporous both the KA of 1.0wt%Pt/ of mesoporous Betazeolite and the 20wt% of the 0.1wt%Pd/ that the catalyzer used is 80wt%.Temperature of reaction and pressure are respectively 230 DEG C and 5Mpa, and the sample after gained upgrading is analyzed according to ASTM-7566 standard method.
Table 1: pyrolysis product distribution in embodiment 1 and comparative example 1
The mass yield of the present embodiment from biomass to aviation fuel is 16%, far above the 7.6wt% in comparative example.The analysis of gained aviation fuel sample is as shown in table 3, and result display is except density is a little more than except jet-A standard, and other all indexs all meet the requirement of this standard to aviation fuel grade.The mode that density index is also in harmonious proportion by the aviation fuel that obtains with embodiment 2 or other aviation fuel is met.
Embodiment 2:
The present embodiment use biomass material be pre-dry corn cob (moisture content <10wt%), use catalyzer for ZnCl
2be 1:1 mixture with the mass ratio of Pt/C, wherein the mass ratio of Pt and C is 0.01:1.Thermocatalysis conversion process is carried out in a fluidized bed reactor.In reaction process, first 200g catalyzer is joined in fluidized-bed, and adopt nitrogen fluidisation to form bubbling bed reactor.Then biomass are incorporated in fluidized-bed by feeding screw, and the speed that biomass are incorporated into fluidized-bed is 100g/h, in 350 DEG C, thermocatalysis conversion reaction occur.The pyrolysis oil gas generated in fluidized-bed enters in condenser and carries out condensation recovery after cyclonic separator separate ash and the catalyzer that carries, uses the condensation of one-level deep cooling to reclaim and to obtain stabilate oil.Gained stabilate oil, except keeping sample analysis, provides follow-up upgrading to react and uses.Analyze through GC/MS, the quality proportion in the stabilate oil that this thermocatalysis conversion process obtains shared by alkyl furan compounds is 84.3%, and wherein the selectivity of 2-methyl furan is 51.4%.
In the present embodiment, stabilate oil carbochain adjustment and hydrogenation deoxidation process carry out respectively.Carbochain adjustment reaction uses sulfuric acid to carry out for catalyzer in the tank reactor of interval, temperature of reaction 60 DEG C, 16 hours reaction times.Carry out oily water separation after having reacted, oil phase provides follow-up hydrogenation deoxygenation to use after drying, and vitriolated aqueous phase is reusable.
Hydrogenation deoxidation reaction is carried out in the high pressure fixed-bed reactor of continuous flow, and aviation fuel presoma pumps into reactor by accurate fresh feed pump, reacts with the catalyzer generation catalysis upgrading being positioned at constant temperature zone.The catalyzer used is Pt/C and Co-Mo/Al
2o
3mixture, loaded catalyst is 20g, wherein, Pt/C and Co-Mo/Al
2o
3mass ratio be the mass ratio of 1:1, Pt and C be 0.01:1, Co/Mo and Al
2o
3mass ratio be 0.02/0.03:1.Reactor inlet temperature is 120 DEG C, and temperature out is 320 DEG C, and reaction pressure is 5Mpa, and the sample after gained upgrading is analyzed according to ASTM-7566 standard method.
The mass yield of the present embodiment from biomass to aviation fuel is 20%, and the analysis of gained aviation fuel sample is as shown in table 3.Result display is except density is a little less than except jet-A standard, and other all indexs all meet the requirement of this standard to aviation fuel grade.The mode that density index is also in harmonious proportion by the aviation fuel that obtains with embodiment 1 or other aviation fuel is met.
Table 3: the detected result of embodiment 1 and embodiment 2 aviation fuel products
Comparative example 1:
The biomass material that this comparative example uses is pre-dry pine wood chip (moisture content <10wt%), and the thermal barrier used is quartz sand.Pyrolytic process carries out in a fluidized bed reactor.In reaction process, 200g sand is joined in fluidized-bed, and adopt nitrogen fluidisation to form bubbling bed reactor.Then biomass are incorporated in fluidized-bed by feeding screw, and the speed that biomass are incorporated into fluidized-bed is 100g/h, in 550 DEG C, pyrolytic reaction occur.The pyrolysis oil gas generated in fluidized-bed enters oil recovery systems after cyclonic separator separate ash and the thermal barrier that carries, is the collection ensureing bio oil, and the mode using the condensation of secondary deep cooling to power up trap carries out reclaiming to obtain bio oil.Gained bio oil, except keeping sample analysis, provides follow-up upgrading to react and uses.Pyrolysis product distribution and the biological oil properties of gained and chemical constitution are as shown in table 1 and table 2.
Table 2: the chemical constitution (based on comprehensive two dimensional gas chromatography and flight time mass spectrum coupling result) of bio oil in embodiment 1 and comparative example
Bio oil upgrading reaction is carried out in the high pressure fixed-bed reactor of continuous flow, and stabilate oil pumps into reactor by accurate fresh feed pump, reacts with the catalyzer generation catalysis upgrading being positioned at constant temperature zone.The catalyzer that catalysis upgrading uses is respectively Pt/C and Co-Mo/Al
2o
3mixture, loaded catalyst is 20g, wherein, Pt/C and Co-Mo/Al
2o
3mass ratio be the mass ratio of 1:1, Pt and C be 0.01:1, Co/Mo and Al
2o
3mass ratio be 0.02/0.03:1.Reactor inlet temperature is 120 DEG C, and temperature out is 320 DEG C, and reaction pressure is 5Mpa.Gained sample after upgrading, after cut cutting, aviation fuel section sample is analyzed according to ASTM-7566 standard method.
The mass yield of this comparative example from biomass to aviation fuel is 7.6%, and gained aviation fuel properties of samples meets aviation fuel standard-required.
Above-described embodiment is only for the invention example is clearly described, and the restriction not to the invention embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.All within the spirit and principles in the present invention any apparent change of extending out or variation be still among the protection domain of the invention claim.
Claims (10)
1. biomass thermal catalyzed conversion and prepare the processing method of aviation fuel, is characterized in that, comprise the steps:
(1) thermocatalysis method for transformation is utilized to be with single oxygen-containing functional group stabilate oil that is feature by Wood Adhesives from Biomass;
(2) design C-C formation reaction, regulate the carbon chain lengths of described stabilate oil, obtain the aviation fuel presoma that carbon chain lengths meets bio-aviation fuel requirement;
(3) described aviation fuel presoma hydrogenation deoxidation preparation meets the bio-aviation fuel of aviation fuel index.
2. biomass thermal catalyzed conversion according to claim 1 and prepare the processing method of aviation fuel, it is characterized in that, in step (1): the catalyzer used in thermocatalysis method for transformation is zeolite molecular sieve, one or more in variable valent metal oxide compound and transition metal salt; Temperature of reaction is 300 DEG C-600 DEG C, and reactor types is pyrolysis form fluidized-bed or the rotating cone of accessible site catalyzer.
3. biomass thermal catalyzed conversion according to claim 2 and prepare the processing method of aviation fuel, is characterized in that, in step (1): temperature of reaction is 400 DEG C-500 DEG C.
4. biomass thermal catalyzed conversion according to claim 1 and prepare the processing method of aviation fuel, it is characterized in that, in step (2): the hydrogenation-alkylated reaction utilizing oxygen-containing functional group to participate in and/or aldol reaction, the carbochain realizing described stabilate oil increases.
5. biomass thermal catalyzed conversion according to claim 4 and prepare the processing method of aviation fuel, it is characterized in that, in step (2): the catalyzer of carbochain reaction of propagation is solid acid catalyst or liquid acid catalyst, and temperature of reaction is 20 DEG C-200 DEG C.
6. biomass thermal catalyzed conversion according to claim 5 and prepare the processing method of aviation fuel, it is characterized in that, in step (2): described solid acid catalyst is zeolite molecular sieve or ion exchange resin, described liquid acid catalyst is sulfuric acid, and temperature of reaction is 60 DEG C-200 DEG C.
7. biomass thermal catalyzed conversion according to claim 1 and prepare the processing method of aviation fuel, it is characterized in that, in step (3): described aviation fuel presoma hydrogenation deoxidation process is petrochemical complex diesel oil hydrogenation workshop section, and catalyzer is Ni-Mo/Al
2o
3, Co-Mo/Al
2o
3with one or more in supported precious metal catalyst.
8. biomass thermal catalyzed conversion according to claim 7 and prepare the processing method of aviation fuel, is characterized in that, in step (3): in hydrogenation deoxidation process, catalyzer is respectively Pt/C and Co-Mo/Al
2o
3mixture, Pt/C and Co-Mo/Al
2o
3mass ratio be the mass ratio of 1:1, Pt and C be 0.01:1, Co/Mo and Al
2o
3mass ratio be 0.02/0.03:1; Reactor inlet temperature is 120 DEG C, and temperature out is 320 DEG C, and reaction pressure is 5Mpa.
9. biomass thermal catalyzed conversion according to claim 1 and prepare the processing method of aviation fuel, it is characterized in that, by aviation fuel presoma hydrogenation deoxidation described in the carbon chain lengths of stabilate oil described in single stage method completing steps (2) and step (3).
10. biomass thermal catalyzed conversion according to claim 9 and prepare the processing method of aviation fuel, it is characterized in that, in the reaction by aviation fuel presoma hydrogenation deoxidation described in the carbon chain lengths of stabilate oil described in single stage method completing steps (2) and step (3), the catalyzer of use is any one in the mesoporous KA of mesoporous Betazeolite and Pt/ of Pd/ or the mixture of the two.
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| CN105331387B (en) | 2018-04-20 |
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